CN116120088A - 一种多孔氧化铝陶瓷的制备方法 - Google Patents
一种多孔氧化铝陶瓷的制备方法 Download PDFInfo
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Abstract
本发明涉及陶瓷材料领域，具体为一种多孔氧化铝陶瓷的制备方法，将铝盐、锆盐、钇盐、加入水中搅拌溶解，再将燃料、铝粉、氮化铝和包覆改性铝粉加入并加热搅拌得到凝胶，将所得凝胶引燃，得到的粉体压制成型后烧结即可，本发明方法所制备多孔氧化铝陶瓷的气孔率＞50％，抗弯强度＞30MPa，在保持较高孔隙率的同时还具有良好的力学性能。
Description
技术领域
本发明涉及陶瓷材料领域，具体为一种多孔氧化铝陶瓷的制备方法。
背景技术
多孔陶瓷是一种材料内部含有大量孔洞(彼此相通或闭合气孔)的无机非金属材料，可利用其较高的表面积和材质本身等特点，应用于各个领域，具有广阔的发展前景。
氧化铝多孔陶瓷是多孔陶瓷材料中尤为重要的一种材料，它不仅具备氧化铝硬度高、耐高温、耐腐蚀、高的电绝缘性与低的介电损耗等特点，以及材料体内较高的比表面积，被广泛应用于气体和液体过滤、净化分离、化工催化载体、生物植入材料、吸声减震和传感器材料等众多领域，并且应用领域迅速拓宽，市场需求量也日益增大，前景非常广阔。
由于多孔氧化铝陶瓷优异的性能和广阔的应用前景，一直受到国内外研究工作者的广泛关注。虽然有很多制备工艺能制备出性能较高的多孔氧化铝陶瓷，但是仍有一些问题需要解决，其中主要问题就是处理好强度与气孔率之间的关系。
发明内容
发明目的：针对上述技术问题，本发明提出了一种多孔氧化铝陶瓷的制备方法。
所采用的技术方案如下：
一种多孔氧化铝陶瓷的制备方法：
将铝盐、锆盐、钇盐、加入水中搅拌溶解，再将燃料、铝粉、氮化铝和包覆改性铝粉加入并加热搅拌得到凝胶，将所得凝胶引燃，得到的粉体压制成型后烧结即可。
进一步地，所述铝盐、锆盐、钇盐为铝、锆、钇的可溶性盐，优选为硝酸盐。
进一步地，所述铝盐、锆盐、钇盐的质量比为300-400：20-40：1-3。
进一步地，所述燃料包括尿素。
进一步地，所述燃料还包括EDTA和柠檬酸。
进一步地，所述包覆改性铝粉为有机硅树脂包覆改性铝粉。
进一步地，所述有机硅树脂包覆改性铝粉的制备方法如下：
取有机硅树脂，搅拌滴加入氨水，滴毕后超声搅拌处理得到溶胶，将铝粉于其中浸渍处理后滤出、干燥即可。
进一步地，所述铝粉、氮化铝的质量比为1-3：1-3。
进一步地，粉体压制成型的压力为10-20MPa。
进一步地，烧结温度为1400-1500℃。
本发明的有益效果：
唐钰栋,白佳海等利用低温燃烧-烧结法制备了多孔Al2O3/ZrO2(Y2O3)陶瓷，发明人以此作为参考，加入高熔点和高硬度的氮化铝颗粒，将其均匀分散在陶瓷基体中，可以使陶瓷基体的位错运动产生钉扎作用，同时，氮化铝与氧化铝膨胀系数存在差别而造成热膨胀失配增韧，由于热膨胀失配，在氮化铝颗粒和氧化铝周围产生残余应力场，因此，在氮化铝颗粒处产生拉应力，而氧化铝晶粒径向处于拉伸状态，其切向处于压缩状态，这时，裂纹倾向于绕过氮化铝颗粒继续扩展，即造成裂纹偏转，从而达到增韧的目的，所制备的多孔氧化铝陶瓷内大面积生长有晶须，经测试为氮化铝晶须，可能是尿素在燃烧时释放的氮气与铝粉反应所生成，其与颗粒状的氮化铝起到复合增韧的效果，而且原位生成的氮化铝晶须可以在陶瓷基体中均匀分散且对孔隙起到良好的支撑作用，对部分铝粉进行有机硅树脂包覆改性，可以保护铝粉避免其过早氧化，而且可以抑制铝粉的爆炸释气和氧化膨胀，使形成的孔隙趋于规则，本发明方法所制备多孔氧化铝陶瓷的气孔率＞50％，抗弯强度＞30MPa，在保持较高孔隙率的同时还具有良好的力学性能。
附图说明
图1为本发明实施例1中所制备多孔氧化铝陶瓷的SEM图。
图2为本发明实施例1中所制备多孔氧化铝陶瓷断面处的SEM图，可以明显看到有氮化铝晶须。
具体实施方式
实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。本发明未提及的技术均参照现有技术。
实施例1：
一种多孔氧化铝陶瓷的制备方法：
将375.1g Al(NO3)3·9H2O、28.5g Zr(NO3)4·5H2O、2.1g Y(NO3)3·6H2O加入650mL水中搅拌溶解，再将由126g尿素、12g EDTA和50g柠檬酸组成的燃料、2g铝粉、1g氮化铝和1.5g有机硅树脂包覆改性铝粉加入并加热搅拌得到凝胶，将所得凝胶放入600℃的马弗炉中加热至燃烧，向收集得到的粉体中加入质量分数为8％的PVA溶液，造粒后在20MPa下压制成型后以5℃/min的速度升温至1480℃烧结2h即可。
其中，有机硅树脂包覆改性铝粉的制备方法如下：
取75mL TM10甲基硅树脂，在搅拌下，滴加入25mL氨水，滴毕后超声搅拌处理8min后得到溶胶，将铝粉于其中浸渍处理后滤出，60℃干燥10h即可。
实施例2：
一种多孔氧化铝陶瓷的制备方法：
将375.1g Al(NO3)3·9H2O、28.5g Zr(NO3)4·5H2O、2.1g Y(NO3)3·6H2O加入650mL水中搅拌溶解，再将由126g尿素、12g EDTA和50g柠檬酸组成的燃料、3g铝粉、3g氮化铝和1.5g有机硅树脂包覆改性铝粉加入并加热搅拌得到凝胶，将所得凝胶放入600℃的马弗炉中加热至燃烧，向收集得到的粉体中加入质量分数为8％的PVA溶液，造粒后在20MPa下压制成型后以5℃/min的速度升温至1500℃烧结2h即可。
其中，有机硅树脂包覆改性铝粉的制备方法同实施例1。
实施例3：
一种多孔氧化铝陶瓷的制备方法：
将375.1g Al(NO3)3·9H2O、28.5g Zr(NO3)4·5H2O、2.1g Y(NO3)3·6H2O加入650mL水中搅拌溶解，再将由126g尿素、12g EDTA和50g柠檬酸组成的燃料、3g铝粉、1g氮化铝和1.5g有机硅树脂包覆改性铝粉加入并加热搅拌得到凝胶，将所得凝胶放入600℃的马弗炉中加热至燃烧，向收集得到的粉体中加入质量分数为8％的PVA溶液，造粒后在20MPa下压制成型后以5℃/min的速度升温至1400℃烧结2h即可。
其中，有机硅树脂包覆改性铝粉的制备方法同实施例1。
实施例4：
一种多孔氧化铝陶瓷的制备方法：
将375.1g Al(NO3)3·9H2O、28.5g Zr(NO3)4·5H2O、2.1g Y(NO3)3·6H2O加入650mL水中搅拌溶解，再将由126g尿素、12g EDTA和50g柠檬酸组成的燃料、1g铝粉、1g氮化铝和1.5g有机硅树脂包覆改性铝粉加入并加热搅拌得到凝胶，将所得凝胶放入600℃的马弗炉中加热至燃烧，向收集得到的粉体中加入质量分数为8％的PVA溶液，造粒后在10MPa下压制成型后以5℃/min的速度升温至1400℃烧结2h即可。
其中，有机硅树脂包覆改性铝粉的制备方法同实施例1。
实施例5：
一种多孔氧化铝陶瓷的制备方法：
将375.1g Al(NO3)3·9H2O、28.5g Zr(NO3)4·5H2O、2.1g Y(NO3)3·6H2O加入650mL水中搅拌溶解，再将由126g尿素、12g EDTA和50g柠檬酸组成的燃料、1g铝粉、3g氮化铝和1.5g有机硅树脂包覆改性铝粉加入并加热搅拌得到凝胶，将所得凝胶放入600℃的马弗炉中加热至燃烧，向收集得到的粉体中加入质量分数为8％的PVA溶液，造粒后在10MPa下压制成型后以5℃/min的速度升温至1500℃烧结2h即可。
其中，有机硅树脂包覆改性铝粉的制备方法同实施例1。
性能测试：
将本发明实施例1-5中所制备的多孔氧化铝陶瓷作为试样；
用Archimedes法测得试样的气孔率；用三点弯曲试验机(跨距为30mm，加载速度为0.5mm/min)测得试样的抗弯强度；
测试结果如下表1所示：
表1
由上表1可知，本发明方法所制备多孔氧化铝陶瓷的气孔率＞50％，抗弯强度＞30MPa，在保持较高孔隙率的同时还具有良好的力学性能。
以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (10)
1.一种多孔氧化铝陶瓷的制备方法，其特征在于，将铝盐、锆盐、钇盐、加入水中搅拌溶解，再将燃料、铝粉、氮化铝和包覆改性铝粉加入并加热搅拌得到凝胶，将所得凝胶引燃，得到的粉体压制成型后烧结即可。
2.如权利要求1所述的多孔氧化铝陶瓷的制备方法，其特征在于，所述铝盐、锆盐、钇盐为铝、锆、钇的可溶性盐，优选为硝酸盐。
3.如权利要求1所述的多孔氧化铝陶瓷的制备方法，其特征在于，所述铝盐、锆盐、钇盐的质量比为300-400：20-40：1-3。
4.如权利要求1所述的多孔氧化铝陶瓷的制备方法，其特征在于，所述燃料包括尿素。
5.如权利要求4所述的多孔氧化铝陶瓷的制备方法，其特征在于，所述燃料还包括EDTA和柠檬酸。
6.如权利要求1所述的多孔氧化铝陶瓷的制备方法，其特征在于，所述包覆改性铝粉为有机硅树脂包覆改性铝粉。
7.如权利要求6所述的多孔氧化铝陶瓷的制备方法，其特征在于，所述有机硅树脂包覆改性铝粉的制备方法如下：
取有机硅树脂，搅拌滴加入氨水，滴毕后超声搅拌处理得到溶胶，将铝粉于其中浸渍处理后滤出、干燥即可。
8.如权利要求1所述的多孔氧化铝陶瓷的制备方法，其特征在于，所述铝粉、氮化铝的质量比为1-3：1-3。
9.如权利要求1所述的多孔氧化铝陶瓷的制备方法，其特征在于，粉体压制成型的压力为10-20MPa。
10.如权利要求1所述的多孔氧化铝陶瓷的制备方法，其特征在于，烧结温度为1400-1500℃。
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